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Triethylamine → 8-Bromo-octanoic acid benzyloxyamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzyloxyamine hydrochloride | HCID 102312 | — |
| 反応物 | Bis(2-oxo-3-oxazolidinyl)phosphinic chloride | HCID 152842 | — |
| 反応物 | 8-Bromooctanoic acid | HCID 548275 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 8-Bromo-octanoic acid benzyloxyamide | HCID 11336403 | 78% |
反応手順
In an ice bath, 14 ml triethylamine was added to a suspension of 3.2 g (20 mmol) O-benzylhydroxylamine hydrochloride in 150 ml dichloromethane. Stirring was continued until the solution became clear. Then, 4.5 g (20 mmol) 8-bromo octanoic acid was added, followed by 5.6 g (22 mmol) bis-(2-oxo-3-oxazolidinyl)-phosphorylchloride. Stirring was continued at ambient temperature for 18 h. The solution was extracted twice with 150 ml each of 1M aqueous hydrochloric acid and twice with 150 ml each of 1M aqueous sodium bicarbonate. The organic solvent was removed i. vac. to give 5.1 g (78%) of 8-bromo-octanoic acid benzyloxyamide as a colorless oil. MS: 330 (M+H+)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091229B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-1345b2679a1f4255af5f660665af3050 |
| 出典メモ | uspto-grants-2006_08 |